Water → 6-(6-amino-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2H)-pyridazinone

HRID 915038노트

반응식

HRID 915038 반응식
[CH:1]([N:4]1[C:9](=[O:10])[CH:8]=[CH:7][C:6]([C:11](=O)[C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=O)=[N:5]1)([CH3:3])[CH3:2].Br.Br.[NH2:23][CH2:24][C:25]([NH2:27])=[NH:26].C[O-].[Na+].O>CO.CCOC(C)=O>[NH2:27][C:25]1[N:26]=[C:11]([C:6]2[CH:7]=[CH:8][C:9](=[O:10])[N:4]([CH:1]([CH3:3])[CH3:2])[N:5]=2)[C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[N:23][CH:24]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 10942334Sodium MethoxideHCID 16211382Aminoacetamidine DihydrobromideHCID 46832460HCID 46832460, 화합물

생성물 1

HCID 693314606-(6-amino-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2H)-pyridazinone수율 7.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 1-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-phenyl-1,2-ethanedione (300 mg), aminoacetamidine dihydrobromide (259 mg) and sodium methoxide (238 mg) in MeOH (3 ml) was stirred for 1.5 hours. Water and EtOAc were added to the reaction mixture. The organic layer was separated, and dried over MgSO4. The solvent was removed in vacuo. The residue was purified by silica gel column chromatography eluted with a mixture of n-hexane and EtOAc. The fractions were concentrated in vacuo to obtain 6-(6-amino-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2H)-pyridazinone (25.6 mg) as white powder.

후처리

  1. customThe organic layer was separated
  2. dry with materialdried over MgSO4
  3. customThe solvent was removed in vacuo
  4. customThe residue was purified by silica gel column chromatography
  5. washeluted with a mixture of n-hexane and EtOAc
  6. concentrationThe fractions were concentrated in vacuo

출처 및 근거

ORD 기록
ord-2f96f97846c44ad391fbe7945cf43dcb
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07265120B2

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